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29Si MAS-NMR Study of Silica Gels and Xerogels: Influence of the Catalyst

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Abstract

Four silica gels were prepared by hydrolysis of tetraethoxysilane (TEOS) in ethanol, using different catalysts: HCl, NaOH, NH3, and NBu4F. Nitrogen adsorption-desorption isotherms indicated that the HCl-catalyzed xerogel was purely microporous, whereas the other samples exhibited a very broad distribution of mesopores and a variable amount of micropores. 29Si MAS NMR spectroscopy of the wet gels (before drying) pointed to a low degree of condensation for the HCl-catalyzed gel, and to the presence of unhydrolyzed TEOS monomer in the NaOH-catalyzed gel. Comparison with the 29Si MAS NMR spectra of the xerogels indicated a significant increase of the degree of condensation during the drying procedure (3 hrs at 120°C under vacuum) for the HCl-catalyzed gel.

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Framery, E., Mutin, P. 29Si MAS-NMR Study of Silica Gels and Xerogels: Influence of the Catalyst. Journal of Sol-Gel Science and Technology 24, 191–195 (2002). https://doi.org/10.1023/A:1015391922572

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